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Potassium Carbonate → Methyl 3-[(4-methyl-5-oxo-2-oxa-4-azabicyclo[4.4.0]deca-6,8,10-trien-9-yl)oxy]-5-[(3S)-1-methyl-2-oxo-pyrrolidin-3-yl]oxy-benzoate

HRID 600559
ノート
印刷プレビュー

反応式

HRID 600559 の反応式
[OH:1][C:2]1[CH:3]=[C:4]([CH:9]=[C:10]([O:12][C@H:13]2[CH2:17][CH2:16][N:15]([CH3:18])[C:14]2=[O:19])[CH:11]=1)[C:5]([O:7][CH3:8])=[O:6].F[C:21]1[CH:30]=[C:29]2[C:24]([C:25](=[O:32])[N:26]([CH3:31])[CH2:27][O:28]2)=[CH:23][CH:22]=1.C(=O)([O-])[O-].[K+].[K+]>C(#N)C>[CH3:31][N:26]1[C:25](=[O:32])[C:24]2[C:29](=[CH:30][C:21]([O:1][C:2]3[CH:3]=[C:4]([CH:9]=[C:10]([O:12][C@H:13]4[CH2:17][CH2:16][N:15]([CH3:18])[C:14]4=[O:19])[CH:11]=3)[C:5]([O:7][CH3:8])=[O:6])=[CH:22][CH:23]=2)[O:28][CH2:27]1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 576631937-Fluoro-3-methyl-2,3-dihydro-4H-1,3-benzoxazin-4-oneHCID 59761136methyl 3-hydroxy-5-[(3S)-1-methyl-2-oxo-pyrrolidin-3-yl]oxy-benzoate2 回

生成物 1

HCID 59761137Methyl 3-[(4-methyl-5-oxo-2-oxa-4-azabicyclo[4.4.0]deca-6,8,10-trien-9-yl)oxy]-5-[(3S)-1-methyl-2-oxo-pyrrolidin-3-yl]oxy-benzoate収率 54%

試薬・触媒・溶媒 1

HCID 6342
Acetonitrile
溶媒

実験手順

A mixture of methyl 3-hydroxy-5-[(3S)-1-methyl-2-oxo-pyrrolidin-3-yl]oxy-benzoate (Intermediate 8) (0.27 g, 1 mmol), 9-fluoro-4-methyl-2-oxa-4-azabicyclo[4.4.0]deca-6,8,10-trien-5-one (CAS no. 915771-24-3) (200 mg, 11 mol) and potassium carbonate (276 g, 2 mmol) in acetonitrile (20 mL) was heated in a microwave at 160° C. for 12 hours. The mixture was evaporated and the residue partitioned between ethyl acetate (40 mL) and water (40 mL). The organic phase was separated, washed with water (10 mL) and brine (20 mL), dried (MgSO4) and evaporated. The aqueous phase was acidified to pH 1 with 2N hydrochloric acid extracted with ethyl acetate (2×30 mL). The combined organic extracts were washed with water (2×20 mL), brine (20 mL), dried (MgSO4) and evaporated. The residue was dissolved in THF (2 mL) and methanol (1 mL) and treated with 2M TMS-diazomethane (0.14 mL) stirred for 30 minutes. The mixture was evaporated and the residue combined with that from the initial extraction and purified by flash chromatography on silica eluting with 0 to 100% ethyl acetate in isohexane to afford the product (232 mg, 54%). 1H NMR δ (300 MHz, CDCl3) 2.10-2.25 (m, 1H), 2.53-2.66 (m, 1H), 2.93 (s, 3H), 3.09 (s, 3H), 3.32-3.58 (m, 2H), 3.89 (s, 3H), 4.91 (t, 1H), 5.17 (s, 2H), 6.51 (s, 1H), 6.72 (d, 1H), 6.97 (s, 1H), 7.34 (s, 1H), 7.52 (s, 1H), 7.93 (d, 1H); m/z 427 (M+H+).

後処理

  1. customThe mixture was evaporated
  2. customthe residue partitioned between ethyl acetate (40 mL) and water (40 mL)
  3. customThe organic phase was separated
  4. washwashed with water (10 mL) and brine (20 mL)
  5. dry with materialdried (MgSO4)
  6. customevaporated
  7. extractionextracted with ethyl acetate (2×30 mL)
  8. washThe combined organic extracts were washed with water (2×20 mL), brine (20 mL)
  9. dry with materialdried (MgSO4)
  10. customevaporated
  11. dissolutionThe residue was dissolved in THF (2 mL)
  12. additionmethanol (1 mL) and treated with 2M TMS-diazomethane (0.14 mL)
  13. customThe mixture was evaporated
  14. extractionextraction
  15. custompurified by flash chromatography on silica eluting with 0 to 100% ethyl acetate in isohexane

出典と根拠

ORDレコード
ord-f05471954af94f27809b81899bc4ee09
出典データセット
uspto-grants-2011_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07902200B2

反応ノート

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このページの内容参加物実験手順後処理出典と根拠反応ノート